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A kind of production method of trigonelline synthetic perfume

A technology for synthesizing fenugreek lactone and fragrances, which is applied in the fields of essential oils/fragrances, fat production, organic chemistry, etc. It can solve the problems of harsh reaction conditions, complicated operations, and low total yield, and meet the requirements of fragrances and high purity. , easy operation effect

Active Publication Date: 2022-05-03
ANHUI HYEA AROMAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some synthetic methods of existing hydroxyfuranones have long routes, high cost, harsh reaction conditions, complicated operation and low overall yield.

Method used

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  • A kind of production method of trigonelline synthetic perfume

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) First feed nitrogen into the 250L reaction kettle with a reflux device for replacement three times, then continue feeding nitrogen to keep the pressure in the kettle at 0.2Mpa.

[0038] (2) After the system pressure is stabilized, add 65kg of anhydrous tetrahydrofuran to the reactor through the anhydrous tetrahydrofuran head tank, after starting the stirrer, add 47kg of diethyl oxalate through the diethyl oxalate head tank, stir evenly, and Diethyl oxalate was well dissolved in THF.

[0039] (3) Open the frozen brine valve, cool the temperature of the reactor to -5°C, and slowly add 104kg of 39% ethylmagnesium bromide-tetrahydrofuran Grignard reagent dropwise through the flow meter in the reactor from the Grignard reagent head tank, Control the reaction temperature at 0~-5°C, and control the dropping time at 2h.

[0040](4) After the dropwise addition, continue to maintain the temperature, stir for 1h, and take a sample for gas chromatography detection. When the co...

Embodiment 2

[0058] (1) First pass nitrogen gas into the 2500L reactor with reflux device for replacement three times, then continue to feed nitrogen gas to maintain the pressure in the kettle at 0.2Mpa.

[0059] (2) After the system pressure is stabilized, add 265kg of anhydrous tetrahydrofuran to the reactor through the anhydrous tetrahydrofuran head tank. After opening the stirrer, add 185kg of diethyl oxalate through the diethyl oxalate head tank, stir evenly, and Diethyl oxalate was well dissolved in THF.

[0060] (3) Open the frozen brine valve, cool the temperature of the reactor to -5°C, slowly add 1240kg13% ethylmagnesium bromide-tetrahydrofuran Grignard reagent dropwise to the reactor through a flow meter from the Grignard reagent head tank, and control The reaction temperature is 0~-5°C, and the dropping time is controlled at 4h.

[0061] (4) After the dropwise addition, continue to maintain the temperature, stir for 2h, and take a sample for gas chromatography detection. When ...

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Abstract

The invention discloses a production method for synthesizing spices from trigonelline, which relates to the technical field of spice production. Anhydrous tetrahydrofuran is used as a solvent, and diethyl oxalate undergoes a Grignard reaction under nitrogen protection conditions, extracted with dichloromethane, washed, After drying over anhydrous sodium sulfate, reclaim dichloromethane for mechanical application, and collect 2-oxobutanoic acid ethyl ester by distillation under reduced pressure; then use absolute ethanol as solvent, under the effect of potassium carbonate and acetaldehyde, 2-oxobutyric acid Carry out cyclization of ethyl ester, recover ethanol under normal pressure, extract and wash with dichloromethane, dry with anhydrous sodium sulfate, recover dichloromethane and apply mechanically, and distill under reduced pressure to obtain trigonelline fragrance product; the process control parameters of the present invention are clear Moreover, the process has good repeatability, the solvent is reasonably recovered and reused, the environmental pollution is reduced and the production cost is reduced at the same time, and the yield and purity of the obtained product trigonelactone are high, which meets the requirements of spices.

Description

Technical field: [0001] The invention relates to the technical field of perfume production, in particular to a production method for synthesizing perfume with trigonelline. Background technique: [0002] Trigonelactone, also known as sugar lactone, chemical name 4,5-dimethyl-3-hydroxy-2(5H)-furanone, the appearance is a transparent light yellow to light yellow liquid, naturally occurring in white sugar, fenugreek , Virginia tobacco, rice wine, tea, coffee and other aroma components, it is the key aroma component of roasted fenugreek seeds, and also an important aroma component in sugar cane sugar residues, with strong and long-lasting fenugreek aroma, caramel Aroma and round-leaved angelica and cherry-like aromas, slightly caramelized fruity aromas, caramel-like aromas at low concentrations, curry-like aromas at high concentrations. [0003] Trigonelline can be used in food spices, and has been approved by the American Food Flavor and Extract Manufacturers Association, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/58C11B9/00
CPCC07D307/58C11B9/0076Y02P20/10
Inventor 王天义徐基龙汪洋张政董金龙汪炎
Owner ANHUI HYEA AROMAS
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